Method of preparing metal oxide-silica composite aerogel and metal oxide-silica composite aerogel prepared by using the same

Patent metadata

Field	Value
Publication number	US-10941043-B2
Application number	US-201615577750-A
Country	US
Kind code	B2
Filing date	Jun 1, 2016
Priority date	Jun 1, 2015
Publication date	Mar 9, 2021
Grant date	Mar 9, 2021

Abstract

Provided are a method of preparing a metal oxide-silica composite aerogel which includes preparing a silicate solution by dissolving water glass at a concentration of 0.125 M to 3.0 M, after adding and mixing a metal salt solution having a metal ion concentration of 0.125 M to 3.0 M to the silicate solution, precipitating metal oxide-silica composite precipitates by adjusting a pH of a resulting mixture to be in a range of 3 to 9, and separating and drying the metal oxide-silica composite precipitates, wherein the metal salt solution includes a magnesium (Mg)-containing metal salt in an amount such that an amount of magnesium ions is greater than 50 mol % based on a total mole of metal ions in the metal salt solution, and a metal oxide-silica composite aerogel having low tap density and high specific surface area prepared by the method.

First claim

The invention claimed is:

1. A method of preparing a metal oxide-silica composite aerogel, the method comprising:
preparing a silicate solution by dissolving water glass at a concentration of 0.125 M to 3.0 M;
adding and mixing a metal salt solution having a metal ion concentration of 0.5 M to 0.8 M to the silicate solution;
precipitating metal oxide-silica composite precipitates by adjusting a pH of a resulting mixture to be in a range of 5.7 or more to less than 7 by adding an acid catalyst;
separating the metal oxide-silica composite precipitates; and
drying the metal oxide-silica composite precipitates by heat treatment or hot air injection to yield the metal oxide-silica composite aerogel,
wherein the metal salt solution comprises a magnesium (Mg)-containing metal salt in an amount such that an amount of magnesium ions is greater than 50 mol % based on a total mole of metal ions in the metal salt solution, and
wherein the metal salt comprises MgCl 2 and CaCl 2 in amounts such that a molar ratio of magnesium ions to calcium ions is in a range of 1.95:1 to 2.1:1.

2. The method of claim 1 , wherein the silicate solution and the metal salt solution are used in amounts such that a molar ratio of water glass:metal ions is in a range of 1:1 to 5:1.

3. The method of claim 1 , wherein the acid catalyst is an inorganic acid.

4. The method of claim 3 , wherein the acid catalyst comprises hydrochloric acid.

5. The method of claim 1 , wherein the metal salt further comprises a salt including at least one metal selected from the group consisting of alkali metals, alkaline earth metals (except magnesium), lanthanides, actinides, transition metals, and Group 13 (IIIA) metals.

6. The method of claim 1 , wherein the drying is performed in a temperature range of 90° C. to 200° C.

7. The method of claim 1 , comprising:
preparing a silicate solution by dissolving water glass at a concentration of 0.125 M to 3.0 M;
adding and mixing a metal salt solution having a metal ion concentration of 0.5 M to 0.8 M to the silicate solution to form a mixture;
precipitating metal oxide-silica composite precipitates by adjusting a pH of the mixture to be in a range of 5.7 or more to less than 7 by adding an acid catalyst; and
separating the metal oxide-silica composite precipitates;
washing the separated metal oxide-silica composite precipitates; and
drying the washed separated metal oxide-silica composite precipitates at 90° C. to 200° C. to yield the metal oxide-silica composite aerogel,

wherein:
the silicate solution and the metal salt solution are used in amounts such that a molar ratio of water glass:metal ions is in a range of 1:1 to 5:1,
the metal salt solution comprises a magnesium (Mg)-containing metal salt in an amount such that an amount of magnesium ions is greater than 50 mol % based on a total mole of metal ions in the metal salt solution, and
the metal salt comprises MgCl 2 and CaCl 2 in amounts such that a molar ratio of magnesium ions to calcium ions is in a range of 1.95:1 to 2.1:1.

8. The method of claim 1 , wherein the metal oxide-silica composite aerogel has a tap density of 0.41 g/ml or less and a Brunauer-Emmett-Teller (BET) specific surface area of 200 m 2 /g or more.

9. The method of claim 8 , wherein the metal oxide-silica composite aerogel has a pore volume in a range of 0.4 cm 3 /g to 1.0 cm 3 /g.

Assignees

• Lg Chemical Ltd

Inventors

• Kim Jong Hun
• Lee Je Kyun

Classifications

• B01J20/02

  comprising inorganic material · CPC title

• C01F5/02

  Magnesia · CPC title

• C01P2006/32

  Thermal properties · CPC title

• C01P2006/14

  Pore volume · CPC title

• C01P2006/11

  Powder tap density · CPC title